Parallel reactor systems and methods for preparing materials

ABSTRACT

Parallel reactor systems for synthesizing materials are disclosed. The reactor systems may include at least two reaction vessels and may be suitable for synthesizing materials produced from corrosive reagents, for example, Ziegler-Natta catalysts. Antechambers may be provided above the reaction vessels to help purge vapors produced by the corrosive reagents. Methods for preparing materials by use of such parallel reactor systems are also disclosed.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a divisional of U.S. application Ser. No.14/388,401, filed on Sep. 26, 2014, which is a national stageapplication of PCT/US2013/033861 under 35 U.S.C. § 371, filed on Mar.26, 2013, which claims the benefit of U.S. Provisional Application No.61/615,666, filed on Mar. 26, 2012, the disclosures of which areincorporated herein by reference in their entirety.

FIELD OF THE DISCLOSURE

The field of the disclosure relates to parallel reactor systems forsynthesizing materials (e.g., catalysts) and, in particular embodiments,for synthesizing materials produced from corrosive reagents. The fieldof the disclosure also relates to methods for preparing materials by useof such parallel reactor systems.

BACKGROUND

Research and development programs directed at discovery of materials usehigh-throughput screening tools to evaluate multiple different candidatematerials and/or process conditions to reduce the costs and timeassociated with the identification of promising candidate materialsand/or process conditions. Various high-throughput parallel reactorsystems have been developed to evaluate multiple candidate materialsand/or process conditions by conducting multiple reactions in parallel(i.e., during the same or overlapping time periods).

A continuing need exists for parallel reactor systems that are capableof processing corrosive components such as components used inZiegler-Natta catalyst synthesis and for methods for preparing materialsby use of such parallel reactor systems.

SUMMARY

One aspect of the present disclosure is directed to a parallel reactorsystem. The system includes a reactor array with at least two reactionvessels. A dispensing system has a needle for dispensing material intothe reaction vessels. An antechamber is disposed above each reactionvessel. The system includes an antechamber sealing member for forming aseal between the needle and the antechamber upon lowering of the needleinto the reaction chamber.

Another aspect of the present disclosure is directed to a method forpreparing a material in one or more reaction vessels of a parallelreactor system. The reactor system includes a reactor array with atleast two reaction vessels, antechambers disposed above each reactionvessel, antechamber sealing members, a valve disposed between eachantechamber and each reaction vessel and an automated dispensing systemfor dispensing material into the reaction vessels. The dispensing systemincludes an injection needle having a tip. The injection needle islowered into an antechamber to form a substantially fluid-tight sealbetween the antechamber sealing member and the injection needle. Theinjection needle is lowered into the reaction chamber and material isdispensed into the reaction vessel. The injection needle is raised toposition the tip of the injection needle in the antechamber. The valveis closed after the tip of the injection needle is positioned in theantechamber. Vapor is purged from the antechamber after the valve isclosed. The injection needle is withdrawn from the antechamber.

Various refinements exist of the features noted in relation to theabove-mentioned aspects of the present disclosure. Further features mayalso be incorporated in the above-mentioned aspects of the presentdisclosure as well. These refinements and additional features may existindividually or in any combination. For instance, various featuresdiscussed below in relation to any of the illustrated embodiments of thepresent disclosure may be incorporated into any of the above-describedaspects of the present disclosure, alone or in any combination.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a perspective view of a reactor system inside an inertatmosphere glove box;

FIG. 2 is a front view of a reactor array and dispensing system;

FIGS. 3-4 are front views of a reactor vessel of the array of FIG. 2 ;

FIG. 5 is a front view of the top plate assembly of the array showing asealing member, antechamber, and valve prior to insertion of aninjection needle;

FIG. 6 is a front view of the top plate assembly of the array showing asealing member, antechamber, and valve upon insertion of the injectionneedle into the antechamber;

FIG. 7 is a front view of the top plate assembly of the array showing asealing member, antechamber, and valve after insertion of the injectionneedle through the open valve;

FIG. 8 is a front view of three alternative sealing members for sealingan antechamber;

FIG. 9 is a perspective view of a reactor array and injection array;

FIG. 10 is a perspective view of the reactor array of FIG. 9 ;

FIG. 11 is a front view of a reaction vessel of the reactor array ofFIG. 9 ;

FIG. 12 is a front view of a dispensing system for injecting fluid intothe reaction vessels;

FIG. 13 is a cross-section perspective view of a waste container sealingmember prior to insertion of an injection needle;

FIG. 14 is a cross-section perspective view of a waste container sealingmember after formation of a seal between the injection needle and ano-ring and prior to the valve opening; and

FIG. 15 is a cross-section perspective view of a waste container sealingmember after the valve is opened and the injection needle is fullypositioned for dispensing waste.

Corresponding reference characters indicate corresponding partsthroughout the drawings.

DETAILED DESCRIPTION

Referring now to FIG. 1 , one embodiment of an automated parallelreactor system is generally designated as 10. The parallel reactorsystem 10 (also referred to herein simply as “reactor system”) includesreactor components such as a parallel reactor array 20 within a housing8 which is commonly referred to in the art as an “inert atmosphere glovebox.” The housing 8 of this embodiment is substantially air-tightrelative to the surrounding ambient. A gas that is inert to thereactants (e.g., nitrogen or argon) may be introduced into the parallelreactor system to insulate the reactants from ambient compounds such aswater vapor or air (particularly oxygen). The inert gas may becontinuously introduced into an inlet and continuously withdrawn throughan outlet (not shown). The housing 8 of this embodiment is pressurizedto prevent ambient gases from entering the housing. Inert gas may betreated to remove potential contaminants (water vapor and/or oxygen) by,for example, treating the gases in a scrubbing device.

The reactor system 10 has three sections—a first section 18, a secondsection (also referred to herein as “main chamber”) 19 and a thirdsection 22. The second section 19 of the housing 8 encloses most reactorsystem components including the reactor arrays, reagents, robotic armsand the like. The first section 18 and third section 22 provideadditional working space for the user and may hold ancillary components.The first section 18 and third section 22 may contain reactor componentssuch as trays and individual containers of reagents, reactor componentssuch as liner vials (i.e., test tubes) and impellers. Such componentsmay be added or removed by use of antechambers 31, 33 which are capableof being isolated from the first section 18 and third section 22.Components may then be added to the antechamber (or removed from theantechamber if components are being removed from the system 10) bypurging the antechambers 31, 33 with inert gas (i.e., at least one cycleof vacuum and flushing with inert gas) and the pressure equivocated withthe first and third sections 18, 22 of the reactor system. Theantechambers 31, 33 may then be opened to the second and third sections18, 22 for adding material to the reaction system 10. The reactor system10 may have less than three sections and, in some embodiments, has onlyone section that contains all reactor system components (i.e., the firstsection 18 and/or third section 22 are optional).

Introducing inert gases into and out of the housing 8 may allow theamount of water vapor in the system 10 to be reduced to less than about10 ppm or even to less than about 1 ppm. Use of the inert gas may alsoallow the amount of oxygen in the system to be reduced to less thanabout 10 ppm or even less than about 1 ppm. However, the reactor systemmay include more or less water vapor and oxygen without departing fromthe scope of the present disclosure. Oxygen and water concentrations inthe inert gas may be measured and, as in some embodiments, are measuredon a semi-continuous or continuous basis.

Referring now to FIG. 2 , a reactor array 20 of the reactor system isshown. The reactor array 20 allows for automated control (and,optionally, individual control) of temperature, pressure and stirringsuch that material (e.g., catalyst) optimization can be performed. Thearray 20 may be housed in the main chamber 19 of the housing 8. Thereactor array 20 includes a number of reaction vessels 9 within areaction block 11 and a top plate assembly 13 that seals the reactionvessels.

The array 20 shown in FIG. 2 includes 8 reaction vessels 9 in a 1×8arrangement. The array 20 may include two reaction vessels 9 or more,such as in other embodiments, about 4 reaction vessels or more, about 8reaction vessels or more, about 16 reaction vessels or more or evenabout 48 reaction vessels or more. The reaction vessels may be in anysuitable arrangement (e.g., 1×8, 2×4, 4×4, etc.).

While the reaction vessels 9 are generally shown in the Figures as beingreaction vials, it should be understood that other vessels (e.g., wellsincluding wells of microtiter plates and the like) may be used withoutdeparting from the scope of the present disclosure.

The reactor array 20 includes an injection array 85 (FIG. 9 ) thatincludes access ports 87 and valves that are used to isolate thecontents of the reaction vessels 9 during material dispensing andreaction mixture sampling.

Referring now to FIG. 10 (the injection array is omitted) the reactorarray includes a heated reactor block 91, and a cooling fluid (e.g., gasor liquid) inlet 92 and a cooling fluid outlet 93. In some embodiments,a liquid is used as the cooling fluid for maximum heat transfer. A fluiddistribution manifold 95 directs cooling fluid around individualreaction vessels 9 so that the temperature within each reaction vesselmay be controlled below ambient temperature. In one embodiment thecooling fluid flux (i.e., the temperature gradient between cooling fluidand the reaction vessel contents) to individual reactors may becontrolled for maximum thermal response.

The reactor array 20 includes a process gas inlet (i.e., inert gasinlet) 82 and outlet 97 for automatic introduction of a process gas thatpressurizes each reaction vessel 9 and provides the ambient for eachvessel. The process gas is also used to automatically introduce an inertgas above the reaction vessels 9 (i.e., in an antechamber as describedbelow) to help insulate the reaction vessels from the rest of the array.Each reaction vessel 9 includes a pressure sensor 99 for measuring andrelaying the pressure in each reaction vessel 9.

The array includes cooling channels 30 (FIG. 3 ) and cooling inlets 27(FIG. 11 ) and cooling outlets 29 associated with each reaction vessel9. The array also includes heated zones 32 (FIG. 3 ) in thermalcommunication with each reaction vessel 9 for controlling thetemperature of the reaction mixture in the vessel. The heated zones 32may be heated by use of a cartridge heater 90 (FIG. 11 ). An externalthermocouple (not shown but its position indicated by “79”) may be usedto indirectly measure the temperature of the reaction contents. Thearray may include insulation to help regulate the temperature of thereaction mixture.

An automated dispensing system 15 (FIG. 2 ) is used to dispense materialinto each reaction vessel 9. The dispensing system 15 is controlled byan arm (not shown) that positions the dispensing system above eachreaction vessel 9 for dispensing of material.

Referring now to FIG. 3 , the contents of the reaction vessels 9 may bestirred by use of a magnetic drive 6 which rotates a magneticallycoupled stirrer 21. The stirrer 21 may include an impeller 24 to promotestirring of the contents of the reaction vessel 9. The rotation of themagnet 6 causes a corresponding magnet in the reaction vessel to rotatealong with a stirrer 21 attached to the magnet thereby stirring thecontents of the reaction vessel 9. In some embodiments and as shown inFIG. 3 , the stirrer 21 extends from an upper end 25 of the reactionvessel 9 and does not contact the walls of the reaction vessel duringuse.

The reactor array may include a dip tube 12 (FIG. 4 ) with a frit 14 ineach reaction vessel 9 to remove fluids from the reaction vessel 9. Thefrit 14 acts to filter solids while withdrawing fluid from the vessel 9.The frit 14 may periodically be backwashed to prevent excess solidmaterial from obstructing the frit 14.

A second tube 16 may be used for injection of solvent. In someembodiments, the tube 16 is eliminated and solvent is introduced throughthe dip tube thereby backwashing the frit 14.

In some embodiments and as shown in FIGS. 3-7 , the parallel reactorsystem includes a sealing member 3 disposed above each reaction vessel9. The sealing member 3 forms a substantially fluid-tight seal betweenan injection needle 50 of the dispensing system 15 (FIG. 2 ).

Suitable alternative sealing members 3 for covering an opening withinthe top plate assembly 13 above the reaction vessel 9 are shown in FIG.8 . A first embodiment of the sealing member 3 is referenced as 3 a inFIG. 8 . Sealing member 3 a is a septum. To dispense material into thereaction vessel 9, the injection needle 50 (FIG. 2 ) is lowered andpierces the septum 3 a. The septum 3 a forms a seal around the injectionneedle and isolates the reaction vessel from the other components of theparallel reactor system. The injection needle continues to be lowered todispense material as further described below.

A second embodiment of the sealing member 3 is referenced as 3 b in FIG.8 . The top plate assembly 13 may include duckbill injectors 3 b thatare seated in the openings within the top plate assembly. To dispensematerial into the reaction vessel 9, the injection needle is lowered andpierces the duckbill injector 3 b. The duckbill injector 3 b forms aseal around the injection needle and isolates the reaction vessel fromthe other components of the parallel reactor system. The injectionneedle continues to be lowered to dispense material as further describedbelow. Once the fluid pressure is reduced, the injector seals whichprevents backflow of fluid.

A third embodiment of the sealing member is referenced as 3 c in FIG. 8. The top plate assembly 13 may include an o-ring 3 c seated in theopenings within the top plate assembly. To dispense material into thereaction vessel 9, the injection needle is lowered through the o-ring 3c thereby forming an air-tight seal with the o-ring. The injectionneedle continues to be lowered to dispense material as further describedbelow. In another embodiment, the sealing member 3 may be a valve (notshown).

In addition to the sealing member 3, the top plate assembly 13 mayinclude antechambers 2 (FIGS. 2-7 ) disposed above each reaction vessel9. The antechambers 2 include inert gas inlets and venting outlets (notshown) for purging the antechamber. Corrosive gases may enter theantechamber 2 during lowering of the needle 50 into the reaction vessel9 (FIGS. 6-7 ). The antechamber 2 allows such gases to be isolated andremoved (and treated downstream) thereby preventing such gases fromcontacting other portions of the parallel reactor system.

In addition to the antechamber 2, the top plate assembly 13 may includea valve 5 (FIGS. 5-7 ) that isolate the antechamber 2 from the reactionvessel 9 when closed. The valve 5 may be controlled by an actuatingmechanism 1. The valve 5 may be closed while the injection needle 50 islowered to engage the sealing member 3 and to enter the antechamber 2.Inert gas may be introduced into the antechamber 2 and withdrawn(optionally while creating a vacuum) to purge the antechamber of anyfluid that is present in the needle. A gas manifold pressure system (notshown) attached to the arm of the dispensing system may seal with a port4 for applying a vacuum and/or applying an inert gas to the antechamber2.

After the antechamber 2 is purged, the valve 5 is opened and the needle50 is lowered toward the reaction chamber 9 (FIG. 7 ) to dispensematerial into the reaction chamber. In embodiments in which the reactionvessel 9 is at a pressure other than ambient, the antechamber 2 ispressurized (or a vacuum is applied) to substantially match the pressureof the reaction chamber 9.

After dispensing of material through the injection needle 50 into thereaction vessel, the injection needle is raised until the tip of theinjection passes through the valve 5 into the antechamber 2. Valve 5 isthen closed and the remaining liquid in the needle is quickly drawn backto behind the first valve 71 of the dispensing system 15 (FIG. 12 ),e.g., by a pump. The antechamber 2 is then purged with inert gas andbrought to ambient pressure to purge any vapor that may be present inthe needle 50. The injection needle 50 may then be further raised andremoved from the top plate assembly 13.

Referring now to FIG. 12 , an embodiment of a dispensing system 15 foruse in dispensing two materials into each reaction vessel is shown. Thesystem 15 includes a first valve 71 used to control flow of a firstfluid (e.g., reaction fluid) through a first supply line 80 and a secondvalve 72 used to control flow of a second fluid (e.g., solvent) througha second supply line 76. The first fluid is generally different than thesecond fluid. The valves may be electronically or pneumaticallyactuated. Allowing two fluids to be dispensed by use of one dispensingsystem reduces cross-contamination (and resulting corrosion) byisolating the corrosive fluid from the surrounding atmosphere andproviding a mechanism for the dispensing system to be rinsed by an inertmaterial.

Other embodiments of the dispensing system utilize additional selectionstyle valve(s) beyond those shown in FIG. 12 . This allows controlledvolumes of different fluids to be contained within a single line andseparated by air gaps. In this manner the exact required amount ofcorrosive fluid can be contained behind the fluid valve described inFIG. 12 , followed by an air gap and a non-corrosive solvent type fluid.Upon dispensing, the fluid valve is actuated and enough volume isdispensed to completely expel the corrosive fluid and a small portion ofthe air gap. After fluid is completely dispensed there is no bulkquantity of the corrosive fluid remaining exposed to the surroundingatmosphere.

The parallel reactor system 10 (FIG. 1 ) may include waste containersfor disposal of unreacted reagents or reaction by-products and othercorrosive materials. In some embodiments and as shown in FIGS. 13-15 ,each waste container may be connected to a sealing assembly to preventmaterial from back filling from the waste container. The waste containersealing assembly includes a sealing member 84 and a valve 77. Thesealing member 84 may, for example, be an o-ring which conforms to thesize and shape of the dispensing needle 75 or the sealing member may bea septum or duck-bill injector as described above in relation to thesealing member 3 (FIG. 8 ) of the reactor array 20 (FIG. 2 ). Thereactor system may include two or more such waste containers to preventthe mixing of two different waste streams which are capable of reactingstrongly when combined. Switching of flow between waste containers maybe achieved by means of selector valve (not shown) which may be actuatedby software control, consistent with chemistry steps to avoid mixing ofincompatible waste streams.

To inject waste into the waste vessel, the waste dispensing needle 75 isplaced through the sealing member 84 to form a primary seal. The valve77 is opened and the needle 75 is lowered past the valve 77. Fluid isinjected into the waste vessel and the dispensing needle 75 is removedfrom the sealing member 84. The valve 77 is closed before the dispensingneedle is removed from the sealing member to prevent back-fill ofmaterial from the waste-containers.

The sealing system may include a port 81 for introducing inert gas tothe waste vessel. An inert purge gas may be continuously fed to thewaste vessel to exclude the surrounding atmosphere and prevent unwantedreaction with that atmosphere. The gas may be treated (e.g., in aneutralization bubbler) and vented (not shown). Neutralization bubblersallow visual verification that venting is occurring. The bubbler mayinclude any liquid (e.g., oil) that may neutralize corrosive gasesand/or hazardous gases. After treatment, gases may be vented through ahood. In some embodiments, the atmosphere is venting continuously.

In some embodiments, the waste containers are positioned outside of themain chamber 19 (FIG. 1 ). The lines between the waste containers andthe main chamber 19 are a potential ingress path for surroundingatmosphere. One or more check valves and/or solenoid valves may be usedto prevent surrounding atmosphere from entering the main chamber 19.Wastes may be removed from the reaction vessels by pressurizing thereaction vessel above the pressure of the waste container (e.g., by useof an inert gas) to cause waste to flow to the waste container andentirely empty into the waste container.

The parallel reactor system 10 (FIG. 1 ) may include a number of armsfor injecting reagent, e.g., automatically injecting reagent, and mayinclude additional reaction vessels, reagent storage and the like. Theparallel reactor system may include various supporting elements forsecuring the components of the system and these supporting elements maybe distinct from one another (similar to the housing sections) or may beintegrally connected in the system. The system may employ variousheating and/or cooling elements for heating and/or cooling the reagentsand/or reaction mixtures. Generally these components may be designed andselected in accordance with the principles and standards within thehigh-throughput parallel processing field. The various components may belinked to a controller (e.g., a microcontroller or computer includingcomputer software) that is configured for automatically operating theparallel reactors, as will be understood by those of skill in the art.

The parallel reactor system 10 described above may be used with reagentsthat are corrosive, and/or to produce reaction products that arecorrosive. The reactor system may be configured to reduce the amount ofcorrosive material that may escape from reagent storage or from thereaction vessel during or after injecting the corrosive material. Forpurposes of the present disclosure, the term “corrosive” includesmaterials that cause oxidation or other weakening of common reactorsystem components causing the components to need to be replaced prior totheir expected useful life. Such corrosive materials include materialsthat themselves are corrosive and/or that may react with ambientmaterials such as water vapor or oxygen or may react with other reactionreagents to create a corrosive material.

In some embodiments of the present disclosure, the parallel reactorsystem 10 is used to produce a solid material in each reaction vesseland, in particular embodiments, is used to produce a heterogeneouscatalyst in each reaction vessel. In some embodiments, the parallelreactor system 10 is used to produce a catalyst commonly known in theart as a Ziegler-Natta catalyst in each reaction vessel. Ziegler-Nattacatalysts are heterogeneous solid-phase catalysts used to producepolyolefins. Ziegler-Natta catalyst may be prepared by use of titaniumchloride (TiCl4) which is a highly corrosive reagent. Preparation mayalso involve use of aluminum chlorides and other chlorine containingreagents. Without preventative measures, these chlorides may result incorrosive films that form in parallel reactor systems including systemswith inert gas insulation (i.e., glove-boxes).

Ziegler-Natta catalysts may be prepared in a series of preparation stepssuch as:

-   -   (a) precursor (e.g., magnesium alkyl) synthesis;    -   (b) preparation of magnesium chloride (MgCl₂) or silica supports        from various precursors;    -   (c) support activation; and    -   (d) TiCl₄ based catalyst synthesis.

It should be noted that the Ziegler-Natta catalyst synthesis stepsdescribed above are exemplary and other routes may be used and/or therecited steps may be eliminated and/or additional preparative stepsincluded. The recited steps should not be considered in a limitingsense.

The Ziegler-Natta catalyst may be prepared in accordance with one ormore methods known to those of skill in the art including, for example,the methods disclosed in U.S. Pat. Nos. 6,730,753; 6,524,995; 7,381,779;7,393,806; 7,687,426; 7,465,775; 6,818,584; 7,666,810; 6,800,581 or U.S.Patent Pub. Nos. 2007/0066772 and 2009/0292089, each of which isincorporated herein by reference for all relevant and consistentpurposes.

Embodiments of the present disclosure have a number of advantages andcapabilities. For example, capabilities include titanation reactionsusing TiCl4, temperature controlled reactions, stir control to avoidattrition of solids, solid/liquid separation and washing and acontrolled inert atmosphere. The proposed synthesis station would allowfor catalyst synthesis on at least two different scales: (1) catalystdiscovery with increased throughput but process control for groups ofreactors and (2) catalyst optimization with moderate throughput andindividual process controlled reactors. Use of a stirrer mounted abovethe reaction vessel enables agitation of reactor vessel contents withoutthe stirrer contacting the walls of the reactor vessel. In contrast,conventional stirrers in similar reactors may result in attrition andbreakage of solid phase components in the reaction vessel due to contactof the impeller with the reactor wall. Accordingly, catalyst morphologymay be preserved (e.g., such as in testing Ziegler-Natta catalysts).Antechambers in the reactor array allow material from the injectionneedle to be purged during and/or after materials are dispensed whichprevents contamination of the other components of the reactor arraywhich is particularly advantageous when corrosive materials are used.

When introducing elements of the present disclosure or the embodiment(s)thereof, the articles “a”, “an”, “the” and “said” are intended to meanthat there are one or more of the elements. The terms “comprising,”“including,” “containing” and “having” are intended to be inclusive andmean that there may be additional elements other than the listedelements. The use of terms indicating a particular orientation (e.g.,“top”, “bottom”, “side”, etc.) is for convenience of description anddoes not require any particular orientation of the item described.

As various changes could be made in the above constructions and methodswithout departing from the scope of the disclosure, it is intended thatall matter contained in the above description and shown in theaccompanying drawing[s] shall be interpreted as illustrative and not ina limiting sense.

What is claimed is:
 1. A method for processing corrosive materials in aparallel reactor system, the parallel reactor system comprising: areactor array comprising at least two reaction vessels; a dispensingsystem having a dispensing needle that dispenses a first corrosive fluidinto each of the at least two reaction vessels; an antechamber disposedabove each of the at least two reaction vessels and comprising a ventingoutlet that purges vapor produced by the first corrosive fluid from theantechamber; an antechamber sealing member associated with each of theat least two reaction vessels; and an actuatable valve between theantechamber and each of the at least two reaction vessels, the methodcomprising: lowering the dispensing needle into the antechamber to forma seal between the antechamber sealing member and the dispensing needle;lowering the dispensing needle into each of the at least two reactionvessels and dispensing the first corrosive fluid into each of the atleast two reaction vessels; raising the dispensing needle to position atip of the dispensing needle in the antechamber; isolating theantechamber from each of the at least two reaction vessels by closingthe actuatable valve, wherein closing the actuatable valve is controlledby an actuating mechanism; purging vapor produced by the first corrosivefluid from the antechamber after the actuatable valve is closed; andwithdrawing the dispensing needle from the antechamber.
 2. The method ofclaim 1, further comprising purging the first corrosive fluid from theantechamber after lowering the dispensing needle into the antechamberand prior to lowering the dispensing needle into each of the at leasttwo reaction vessels.
 3. The method of claim 1, further comprisingdispensing a second fluid into each of the at least two reactionvessels.
 4. The method of claim 1, wherein the parallel reactor systemfurther comprises a waste container and a sealing assembly having asealing member and a valve disposed between the sealing member and thewaste container, the method comprising: forming a seal between thesealing member and the dispensing needle; opening the valve after theseal has formed between the dispensing needle and the sealing member;dispensing waste from the dispensing needle into the waste container;closing the valve after waste has been dispensed into the wastecontainer; and withdrawing the dispensing needle after the valve hasbeen closed.
 5. The method of claim 1, wherein the parallel reactorsystem forms a Ziegler-Natta catalyst by: (1) synthesizing a magnesiumalkyl precursor; (2) preparing a magnesium chloride support from themagnesium alkyl precursor; (3) activating the magnesium chloridesupport; and (4) contacting the magnesium chloride support with titaniumchloride (TiCl₄).
 6. The method of claim 1, wherein the parallel reactorsystem comprises at least two waste containers, the method comprisingdispensing a different waste material to each of the at least two wastecontainers.
 7. The method of claim 2, wherein the first corrosive fluidis purged from the antechamber by circulating inert gas through theantechamber.
 8. The method of claim 3, wherein the second fluid iscorrosive.